CN113893303A - Preparation method of rhizoma paridis extract - Google Patents
Preparation method of rhizoma paridis extract Download PDFInfo
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- CN113893303A CN113893303A CN202111139355.5A CN202111139355A CN113893303A CN 113893303 A CN113893303 A CN 113893303A CN 202111139355 A CN202111139355 A CN 202111139355A CN 113893303 A CN113893303 A CN 113893303A
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- paris polyphylla
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- 239000000284 extract Substances 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 241000244987 Daiswa polyphylla Species 0.000 claims abstract description 113
- 238000000605 extraction Methods 0.000 claims abstract description 74
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000000843 powder Substances 0.000 claims abstract description 59
- 239000002904 solvent Substances 0.000 claims abstract description 53
- 238000010992 reflux Methods 0.000 claims abstract description 44
- 239000000243 solution Substances 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 239000000706 filtrate Substances 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 230000009286 beneficial effect Effects 0.000 abstract description 6
- 238000010828 elution Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 230000008595 infiltration Effects 0.000 description 4
- 238000001764 infiltration Methods 0.000 description 4
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- 239000000047 product Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 238000004364 calculation method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003480 eluent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000855 fermentation Methods 0.000 description 2
- 230000004151 fermentation Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
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- 238000011069 regeneration method Methods 0.000 description 2
- 238000004366 reverse phase liquid chromatography Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 241000186361 Actinobacteria <class> Species 0.000 description 1
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 244000063299 Bacillus subtilis Species 0.000 description 1
- 235000014469 Bacillus subtilis Nutrition 0.000 description 1
- 206010010904 Convulsion Diseases 0.000 description 1
- 241000234280 Liliaceae Species 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical group O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 description 1
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- 239000012153 distilled water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003571 electronic cigarette Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
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- IUCHKMAZAWJNBJ-RCYXVVTDSA-N oleanolic acid 3-O-beta-D-glucosiduronic acid Chemical compound O([C@H]1CC[C@]2(C)[C@H]3CC=C4[C@@]([C@@]3(CC[C@H]2C1(C)C)C)(C)CC[C@]1(CCC(C[C@H]14)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O IUCHKMAZAWJNBJ-RCYXVVTDSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 1
- 229930182490 saponin Natural products 0.000 description 1
- 150000007949 saponins Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a preparation method of a paris polyphylla extract, and relates to the field of paris polyphylla extraction technology. The preparation method of the paris polyphylla extract comprises the following steps of mixing and infiltrating: uniformly mixing the rhizoma paridis powder and a solvent according to the weight ratio of 1 (9-15) to obtain a mixed solution; reflux extraction: extracting the mixed solution for 1.5-2.5 h under reflux, filtering to obtain A filter residue and A filtrate, mixing the A filter residue with a solvent, extracting for 0.8-1.2 h under reflux, and filtering to obtain B filtrate; concentrating and preparing: and combining the filtrate A and the filtrate B to obtain a combined solution, and concentrating the combined solution to obtain the paris polyphylla extract. The method reduces the extraction steps by controlling the weight ratio of the rhizoma paridis powder to the ethanol, can reduce the loss caused by multiple filtering, elution and other steps, is beneficial to improving the yield of the rhizoma paridis extract, has less extraction steps, mild reaction conditions and strong operability, and is convenient for industrial preparation of the rhizoma paridis extract.
Description
Technical Field
The invention relates to the field of a paris polyphylla extraction technology, in particular to a preparation method of a paris polyphylla extract.
Background
Rhizoma paridis is a precious Chinese medicinal material, and is dried rhizome of Yunnan rhizoma paridis or Paris polyphylla Smith of Liliaceae. Rhizoma paridis is bitter in taste, slightly cold in nature and slightly toxic, and has the effects of clearing away heat and toxic materials, relieving swelling and pain, cooling liver and arresting convulsion. Through the development of many years, the paris polyphylla is used not only in medicines, but also in a plurality of health care products. The extract of the paris polyphylla is generally added into a health-care product, so that the health-care effect of the health-care product can be improved.
Before the paris polyphylla is used for preparing a health-care product, a proper preparation method needs to be selected to prepare the paris polyphylla extract. In the related technology, paris polyphylla strain is fermented for a period of time, water is filtered out, sterilization treatment is carried out, microwave heating reflux extraction is carried out, the extract is decolored, degreased, decompressed, concentrated and centrifugally precipitated, the obtained supernatant is passed through a macroporous adsorption resin column and eluted by ethanol solution, then the ethanol eluent is concentrated and separated by adopting reversed phase liquid chromatography to obtain ethanol and extract, and the obtained extract is crystallized and dried to obtain paris polyphylla extract.
In view of the above related technologies, the inventors believe that in the above preparation method, the paris polyphylla needs to be subjected to multiple steps of fermentation, reflux extraction, filtration, decolorization and degreasing, concentration and precipitation, elution, separation, crystallization and the like to prepare the paris polyphylla extract, which easily causes excessive loss of the paris polyphylla extract and is not beneficial to improving the yield of the paris polyphylla extract.
Disclosure of Invention
In order to solve the problem of excessive loss of the paris polyphylla extract, the application provides a preparation method of the paris polyphylla extract.
The preparation method of the paris polyphylla extract adopts the following technical scheme:
a method for preparing rhizoma paridis extract comprises the following steps,
mixing and infiltrating: uniformly mixing the rhizoma paridis powder and a solvent according to the weight ratio of 1 (9-15) to obtain a mixed solution;
reflux extraction: extracting the mixed solution for 1.5-2.5 h under reflux, filtering to obtain A filter residue and A filtrate, mixing the A filter residue with a solvent, and extracting for 0.8-1.2 h under reflux to obtain B filtrate;
concentrating and preparing: and combining the filtrate A and the filtrate B to obtain a combined solution, and concentrating the combined solution to obtain the paris polyphylla extract.
The application optimizes the weight ratio of the rhizoma paridis powder to the solvent through experiments, and the inventor finds that the weight ratio of the rhizoma paridis powder to the ethanol is controlled within the range of 1 (9-15), so that effective substances in the rhizoma paridis powder can be conveniently dissolved in the solvent, and the rhizoma paridis extract can be obtained by directly performing reflux extraction and concentration after the rhizoma paridis powder and the solvent are mixed and soaked under the above conditions. According to the method, the weight ratio of the rhizoma paridis powder to the ethanol is controlled, the extraction steps are reduced, the loss caused by multiple filtering, elution and other steps can be reduced, the yield of the rhizoma paridis extract is improved, the extraction steps are few, the reaction conditions are mild, the operability is high, and the industrial preparation of the rhizoma paridis extract is facilitated.
Preferably, in the step of mixing and infiltrating, the paris polyphylla powder and the solvent are mixed, stirred for 1-5 min every 5-15 min, and mixed for 0.8-1.5 h to obtain a mixed solution.
After the paris polyphylla powder is mixed with the solvent, the effective substances in the paris polyphylla powder can be gradually dissolved in the solvent, but after the effective substances are dissolved for a period of time, the concentration of the effective substances is higher around the paris polyphylla powder particles, so that the effective substances are inconvenient to be continuously dissolved in the solvent. The method of the application is characterized in that the mixed solution is stirred for one time at intervals, so that the effective substances dissolved in the solvent are conveniently dispersed in the solvent, the concentration of the effective substances around the particles of the rhizoma paridis powder is reduced, the residual effective substances in the rhizoma paridis powder are favorably dissolved in the solvent, the dissolving time can be shortened, and the yield and the extraction efficiency of the rhizoma paridis extract are conveniently improved.
Preferably, the weight ratio of the rhizoma paridis powder in the mixed infiltration step to the solvent in the reflux extraction step is 1 (5-12).
Because the filter residue A also contains effective substances, the method can improve the yield of the paris polyphylla extract by carrying out secondary extraction on the filter residue A and the solvent. The application optimizes the dosage of the solvent in the secondary extraction through experiments, and the inventor finds that the dosage of the solvent is controlled within the range, so that the effective substances in the filter residue A can be conveniently extracted, and the yield of the paris polyphylla extract can be further improved.
Preferably, in the concentration step, the weight of the paris polyphylla extract is 21-25% of the weight of the combined solution.
The excessive solvent contained in the extract can cause the extract not to meet the use condition, and the concentration time is too long, thus being not beneficial to improving the extraction efficiency. The inventor finds that when the weight ratio of the solvent in the reflux extraction step to the rhizoma paridis powder in the mixed infiltration step is in the range of 1 (5-12), the combined solution is concentrated to 21% -25% of the original weight, the rest extract is basically free of liquid drops and is in a paste shape, the yield of the obtained extract is high, and the obtained extract meets the use requirement of the electronic cigarette liquid, shortens the concentration time and is convenient to improve the extraction efficiency.
Preferably, the fineness of the rhizoma paridis powder is 20-60 meshes.
The powder can be agglomerated in the solution, the powder is agglomerated together, and the outside and the inside of the powder agglomerate are heated unevenly in the heating process, so that the powder is easily burnt. When the weight ratio of the paris polyphylla powder to the solvent is controlled within the range of 1 (9-15), the paris polyphylla powder is controlled to be 20-60 meshes, gaps among paris polyphylla powder particles are large, agglomeration is not prone to occurring, the solvent can conveniently soak the paris polyphylla powder particles, and effective substances in the paris polyphylla powder can be dissolved in the solvent.
Therefore, the paris polyphylla powder is controlled to be 20-60 meshes, and the agglomeration of the paris polyphylla powder in the reflux extraction process can be reduced, so that the scorching phenomenon caused by uneven heating of the paris polyphylla powder is reduced, and the yield of the paris polyphylla extract is further improved conveniently.
Preferably, the solvent is ethanol with the concentration of 85-95%.
According to the method, the ethanol with the concentration of 85% -95% is used as the solvent, the boiling point of the ethanol is low, the reaction condition is mild, and potential safety hazards can be reduced in the reflux extraction process; when the concentration of the industrial alcohol exceeds 95%, the preparation is difficult, the method selects the ethanol with the concentration of 85% -95%, the production is easy in industrial production, the industrial extraction of the paris polyphylla extract is convenient, and the extraction cost is reduced; in addition, in the concentration preparation step, the ethanol is easily separated from the paris polyphylla extract, so that the paris polyphylla extract is conveniently obtained.
Preferably, in the reflux extraction step, the reflux extraction temperature is 78-85 ℃.
When the temperature of reflux extraction is too high, the effective components dissolved in ethanol are easily damaged; when the temperature of reflux extraction is too low, the effective substances in the rhizoma paridis powder are not favorably dissolved in ethanol; because the boiling point of the ethanol at normal pressure is 78 ℃, the method controls the temperature of reflux extraction within the range, the evaporation speed of the ethanol is moderate, the damage to effective substances is small, and the method is favorable for improving the yield of the paris polyphylla extract.
Preferably, in the concentration preparation step, the concentration is carried out in the pressure of-0.08 to-0.12 MPa, and the temperature in the concentration process is 52 to 62 ℃.
The boiling point of ethanol can be lowered by reducing the pressure during the concentration process. The pressure and the temperature in the concentration process are optimized through experiments, and the inventor finds that the pressure in the concentration process is controlled within the range of-0.08 MPa to-0.12 MPa, and the temperature in the concentration process is controlled within the range of 52 ℃ to 62 ℃, so that the method is favorable for improving the yield of the paris polyphylla extract.
In summary, the present application has the following beneficial effects:
1. according to the method, the weight ratio of the rhizoma paridis powder to the ethanol is controlled, so that the extraction steps are reduced, the loss caused by multiple filtering, elution and other steps can be reduced, the yield of the rhizoma paridis extract is improved, the extraction steps are few, the reaction conditions are mild, the operability is high, and the industrial preparation of the rhizoma paridis extract is facilitated.
2. The fineness of the paris polyphylla powder in the application is 20-60 meshes, and the agglomeration of the paris polyphylla powder in the reflux extraction process can be reduced, so that the scorching phenomenon caused by uneven heating of the paris polyphylla powder is reduced, and the yield of the paris polyphylla extract is further improved conveniently.
3. The solvent is 85% -95% ethanol, is convenient to obtain, and is beneficial to reducing the extraction cost, and in the concentration preparation step, the ethanol is easy to separate from the paris polyphylla extract, so that the paris polyphylla extract is convenient to obtain.
Detailed Description
The present application will be described in further detail with reference to examples.
The rhizoma paridis powder in the invention is prepared by crushing the rhizome of rhizoma paridis Yunnanensis with the water content of 30 percent.
Examples
Examples 1 to 7
As shown in Table one, examples 1-7 differ in the weight ratio of Paris polyphylla powder to solvent. Wherein the first part of solvent and the second part of solvent are both ethanol with the concentration of 95 percent.
The following will explain in detail by taking example 1 as an example.
The method of preparing the paris polyphylla extract of embodiment 1, comprising the steps of:
mixing and infiltrating: weighing the paris polyphylla powder with the fineness of 20-40 meshes and a first part of solvent according to the proportion, putting the paris polyphylla powder and the first part of solvent into a mixer, stirring for 3min every 10min, and mixing for 1h to obtain a mixed solution;
reflux extraction: adding the mixed solution into a reflux extraction device, keeping the temperature in the reflux extraction device at 80 ℃, performing reflux extraction for 2 hours to obtain an extracting solution A, filtering the extracting solution A by using a suction filter to obtain a filter residue A and a filtrate A, adding the filter residue A and a second part of solvent into the reflux extraction device, keeping the temperature in the reflux extraction device at 80 ℃, performing reflux extraction for 1 hour to obtain an extracting solution B, and filtering the extracting solution B by using the suction filter to obtain a filtrate B;
concentrating and preparing: adding the filtrate A and the filtrate B into a reaction kettle to obtain a combined solution, keeping the pressure in the reaction kettle at-0.1 MPa and the temperature at 57 ℃, concentrating the combined solution, testing the residual weight of the combined solution in the concentration process, stopping concentrating when the residual weight is 23% of the original weight of the combined solution, and obtaining the residual paste, namely the paris polyphylla extract.
Watch 1
Example 8
The difference between the embodiment and the embodiment 2 is that the fineness of the rhizoma paridis powder is 40-60 meshes.
Example 9
The difference between the embodiment and the embodiment 2 is that the fineness of the rhizoma paridis powder is 60-80 meshes.
Example 10
The difference between the embodiment and the embodiment 2 is that the fineness of the rhizoma paridis powder is 10-20 meshes.
Example 11
This example differs from example 2 in that the solvent is ethanol at a concentration of 90%.
Example 12
This example differs from example 2 in that the solvent is ethanol at a concentration of 85%.
Example 13
This example differs from example 2 in that the solvent is ethanol at a concentration of 80%.
Example 14
The difference between this example and example 2 is that when the remaining weight of the combined solution is 21% of the original weight of the combined solution, the concentration is stopped and the remaining paste is the extract of rhizoma paridis.
Example 15
The difference between this example and example 2 is that when the remaining weight of the combined solution is 25% of the original weight of the combined solution, the concentration is stopped and the remaining paste is the extract of rhizoma paridis.
Example 16
The difference between this example and example 2 is that when the remaining weight of the combined solution is 20% of the original weight of the combined solution, the concentration is stopped and the remaining paste is the extract of rhizoma paridis.
Example 17
The difference between this example and example 2 is that when the remaining weight of the combined solution is 26% of the original weight of the combined solution, the concentration is stopped and the remaining paste is the extract of rhizoma paridis.
Example 18
The difference between this example and example 2 is that in the step of mixing and infiltrating, the paris polyphylla powder and the first portion of solvent are put into a mixer, stirred for 1min every 5min, and mixed for 0.8h to obtain a mixed solution.
Example 19
The difference between this example and example 2 is that in the step of mixing and infiltrating, the paris polyphylla powder and the first portion of solvent are put into a mixer, stirred for 5min every 15min, and mixed for 1.5h to obtain a mixed solution.
Example 20
This example is different from example 2 in that in the step of mixing and infiltrating, the paris polyphylla powder and the first portion of solvent are put into a mixer and stirred continuously for 1 hour to obtain a mixed solution.
Example 21
This example is different from example 2 in that in the reflux extraction step, the temperature in the reflux extraction apparatus was maintained at 78 ℃.
Example 22
This example is different from example 2 in that in the reflux extraction step, the temperature in the reflux extraction apparatus was maintained at 85 ℃.
Example 23
This example is different from example 2 in that in the reflux extraction step, the temperature in the reflux extraction apparatus was maintained at 76 ℃.
Example 24
This example is different from example 2 in that in the reflux extraction step, the temperature in the reflux extraction apparatus was maintained at 87 ℃.
Example 25
This example is different from example 2 in that in the concentration preparation step, the pressure in the reaction vessel was maintained at-0.08 MPa and the temperature was maintained at 62 ℃.
Example 26
This example is different from example 2 in that in the concentration preparation step, the pressure in the reaction vessel was maintained at-0.12 MPa and the temperature was maintained at 52 ℃.
Example 27
This example is different from example 2 in that in the concentration preparation step, the pressure in the reaction vessel was maintained at-0.06 MPa and the temperature was maintained at 70 ℃.
Example 28
This example is different from example 2 in that in the concentration preparation step, the pressure in the reaction vessel was maintained at-0.14 MPa and the temperature was maintained at 45 ℃.
Comparative example
Comparative example 1
The comparative example provides a method for extracting and purifying rhizoma paridis saponin I from rhizoma paridis, which comprises the following steps:
s1: crushing rhizoma paridis into coarse powder, placing into a closed container, inoculating strains, fermenting at 60 deg.C for 48 hr, wherein the strains are composition of yeast, actinomycetes, Bacillus subtilis, and Bacillus, washing with sterile distilled water for 3 times after fermentation, draining water, sterilizing, adding 9 times of 95% ethanol, extracting under reflux for 15min for 2 times under microwave heating, controlling reflux heating temperature to 95 deg.C by controlling microwave irradiation amount, filtering, and mixing extractive solutions;
s2: decolorizing the extractive solution of step S1 with activated carbon, defatting with acetone, placing in a rotary evaporator at 65 deg.C, reducing pressure to 0.02MPa, and concentrating until the content of rhizoma paridis saponin is 15%; adding 85% ethanol solution into the concentrated solution, continuously centrifuging for 3 times in a centrifuge of 3000r/min, and mixing the supernatants;
s3: and (3) passing the supernatant obtained in the step S2 through a D101 macroporous adsorption resin column under the conditions that: the analytical agent is 58% ethanol solution, the dosage of the analytical agent is 3.2 times of the volume of the macroporous adsorption resin, the regeneration solvent is 3.5% KOH solution, the flow rate of an adsorption area is 10BV/h, the flow rate of a desorption area is 20BV/h, the flow rate of a regeneration area is 10BV/h, the switching time is 650s, the temperature is 60 ℃, the pressure is 0.1MPa, 55% and 80% ethanol solutions are sequentially used for elution, 80% ethanol eluent is collected, and concentrated solution is obtained through concentration;
s4: separating the concentrated solution obtained in step S3 by reverse phase liquid chromatography to obtain ethanol and extract, recovering ethanol, crystallizing the obtained extract at 16 deg.C, drying at 70 deg.C for 3 hr to obtain parinuin I with purity of 98.5%, and yield of 2.5%.
Comparative examples 2 to 3
As shown in Table two, comparative examples 2 to 3 are different from example 1 in that the weight ratio of the Paris polyphylla powder, the first part of the solvent and the second part of the solvent is different.
Watch two
Performance test
Yield calculation
The paris polyphylla extract obtained in examples 1-28 and comparative examples 2-3 is put into an oven and dried for 3 hours at 70 ℃ to obtain a solid extract, and the weight ratio of the solid extract to the paris polyphylla powder in the mixed infiltration step is the yield of the paris polyphylla extract, and the result is shown in table three.
Purity calculation
Sequentially collecting the extract of Paris polyphylla obtained in examples 1-28 and comparative examples 1-3, and adding into high performance liquid chromatography under InertsilODS-3C18 chromatographic column (150mm × 4.6mm, 5 μm); the mobile phase is acetonitrile-water (45: 55); the detection wavelength is 210 nm; the flow rate was 1.0 mL/min-1(ii) a The column temperature was 35 ℃; the amount of the sample was 20.0. mu.L. The purity of the paris polyphylla extract is calculated by an area normalization method, and the result is shown in table three.
Calculation of extraction efficiency
The time spent from the beginning of the experiment to the end of the experiment in the examples 1 to 28 and comparative examples 1 to 3 was calculated in order, in minutes, the shorter the time spent, the higher the extraction efficiency, and the results are shown in table three.
Watch III
The present application is described in detail below with reference to the test data provided in table three.
Example 1 and comparative example 1 are compared for the extraction process of the paris polyphylla extract. It can be seen that the purity of the paris polyphylla extract obtained in example 1 is not much different compared to that of comparative example 1, but the yield and extraction efficiency of the paris polyphylla extract of example 1 are significantly improved. This shows that, under the preparation method of the present application, the significant improvement of the yield and extraction efficiency of the paris polyphylla extract is facilitated.
Examples 1-3 and comparative examples 2-3 are compared for the weight ratio of Paris polyphylla powder to the first portion of solvent. It can be seen that, compared with example 1, in examples 2 to 3, the purity and extraction efficiency of the obtained paris polyphylla extract were not greatly changed, and the yield was high; the purity and extraction efficiency of the paris polyphylla extract obtained in comparative examples 2-3 did not vary much, but the yield was significantly reduced. This shows that when the mass ratio of the paris polyphylla powder to the first solvent is in the range of 1 (9-15), the method is favorable for improving the yield of the paris polyphylla extract.
Example 2 and examples 4-7 are compared for the weight ratio of paris polyphylla powder to the second portion of solvent. It can be seen that the purity and extraction efficiency of the paris polyphylla extracts of examples 4-7 did not change much compared to example 2, but the variation in the yield of the paris polyphylla extracts of examples 4 and 5 was small, the yields of the paris polyphylla extracts of examples 6 and 7 were significantly reduced, and the yields of the paris polyphylla extracts of examples 4 and 5 were smaller. This shows that the weight ratio of the rhizoma paridis powder to the second solvent is in the range of 1 (5-12), which is helpful for further increasing the yield of the rhizoma paridis extract.
Example 2 and examples 8-10 are compared for the weight ratio of paris polyphylla powder to the second portion of solvent. It can be seen that, compared to example 2, the extract of paris polyphylla obtained in example 8 has little variation in yield, purity and extraction efficiency, the extract of paris polyphylla obtained in example 9 has little variation in yield and purity, and the extract of paris polyphylla obtained in example 10 has little variation in yield and purity. This indicates that the fineness of the Paris polyphylla powder is in the range of 20-60 mesh, which is helpful for improving the yield of the Paris polyphylla extract, and when the fineness of the Paris polyphylla powder is more than 60 mesh, it is not beneficial to improve the purity of the Paris polyphylla extract.
Example 2 and examples 11-13 are compared for solvent concentration. It can be seen that the yields of the paris polyphylla extracts obtained in examples 11-13 were sequentially decreased and the yield of the paris polyphylla extract obtained in example 13 was the smallest compared to example 2. This shows that when ethanol is used as the solvent, increasing the concentration of ethanol is helpful to increase the yield of the paris polyphylla extract, and when the concentration of ethanol is in the range of 85-95%, the extraction effect of paris polyphylla powder is better.
Example 2 and examples 14-17 are compared for the weight ratio of the paris polyphylla extract to the original weight of the combined liquid. It can be seen that the yields of examples 14 to 17 do not change much compared to example 2, but the extraction efficiencies of examples 14 and 16 decrease in order, the purities of examples 14 and 16 increase in order, the extraction efficiencies of examples 15 and 17 increase in order, and the purities of the paris polyphylla extracts obtained in examples 15 and 17 decrease in order. This shows that the increase of the weight ratio of the paris polyphylla extract to the original weight of the combined liquid easily results in lower extraction efficiency, the decrease of the weight ratio of the paris polyphylla extract to the original weight of the combined liquid easily results in lower purity of the paris polyphylla extract, and when the weight ratio of the paris polyphylla extract to the original weight of the combined liquid is 21-25%, both the extraction efficiency and the purity of the paris polyphylla extract can be maintained in a larger range of values.
Example 2 and examples 18-20 were compared for the interval between stirring in the mixed infiltration step. It can be seen that the yields, purities and extraction efficiencies of the paris polyphylla extracts of examples 18-20 did not vary much as compared to example 2. This shows that the stirring conditions of example 2 and examples 18-20 all contribute to the improvement of the yield, purity and extraction efficiency of the paris polyphylla extract.
Example 2 and examples 21-24 were compared for extraction temperature in the reflux extraction step. It can be seen that the yields, purities and extraction efficiencies of the paris polyphylla extracts of examples 21 and 22 were not greatly changed, the yield of the paris polyphylla extract of example 23 was significantly reduced and the purity of the paris polyphylla extract of example 24 was less compared to example 2. This shows that the reflux extraction step helps to increase the yield and purity of the Paris polyphylla extract when the extraction temperature is between 78-85 deg.C.
Example 2 and examples 25-28 are compared against the concentration conditions in the concentration preparation step. It can be seen that the yields and purities of the paris polyphylla extracts of examples 25 and 26 were not changed much, the yields of examples 27 and 28 were less, the extraction efficiencies of examples 25 and 27 were lower, and the extraction efficiencies of examples 26 and 28 were higher, compared to example 2. This shows that when the concentration pressure in the concentration preparation step is-0.08 to-0.12 MPa and the temperature is 52 to 62 ℃, the yield and the extraction efficiency of the paris polyphylla extract can be improved.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (8)
1. A preparation method of a rhizoma paridis extract is characterized in that: comprises the following steps of (a) carrying out,
mixing and infiltrating: uniformly mixing the rhizoma paridis powder and a solvent according to the weight ratio of 1 (9-15) to obtain a mixed solution;
reflux extraction: extracting the mixed solution for 1.5-2.5 h under reflux, filtering to obtain A filter residue and A filtrate, mixing the A filter residue with a solvent, extracting for 0.8-1.2 h under reflux, and filtering to obtain B filtrate;
concentrating and preparing: and combining the filtrate A and the filtrate B to obtain a combined solution, and concentrating the combined solution to obtain the paris polyphylla extract.
2. The method for preparing the paris polyphylla extract as claimed in claim 1, wherein the steps of: in the step of mixing and infiltrating, the paris polyphylla powder and the solvent are mixed, stirred for 1-5 min every 5-15 min and mixed for 0.8-1.5 h to obtain a mixed solution.
3. The method for preparing the paris polyphylla extract as claimed in claim 1, wherein the steps of: the weight ratio of the rhizoma paridis powder in the step of mixing and infiltrating and the solvent in the step of reflux extraction is 1 (5-12).
4. The method for preparing the paris polyphylla extract as claimed in claim 3, wherein the steps of: in the concentration preparation step, the weight of the paris polyphylla extract is 21-25% of the weight of the combined solution.
5. The method for preparing the paris polyphylla extract as claimed in claim 3, wherein the steps of: the rhizoma paridis powder is 20-60 meshes.
6. The method for preparing the paris polyphylla extract as claimed in claim 1, wherein the steps of: the solvent is ethanol with the concentration of 85% -95%.
7. The method for preparing the paris polyphylla extract as claimed in claim 6, wherein the steps of: in the reflux extraction step, the temperature of reflux extraction is 78-85 ℃.
8. The method for preparing the paris polyphylla extract as claimed in claim 6, wherein the steps of: in the concentration preparation step, concentration is carried out in-0.08 to-0.12 MPa, and the temperature in the concentration process is 52 to 62 ℃.
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| CN1899491A (en) * | 2006-06-30 | 2007-01-24 | 浙江大学 | Method for preparing paris polyphylla total saponin and its use |
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| CN1899491A (en) * | 2006-06-30 | 2007-01-24 | 浙江大学 | Method for preparing paris polyphylla total saponin and its use |
| CN107619427A (en) * | 2017-11-03 | 2018-01-23 | 隆安县荣胜养殖有限公司 | A kind of method of the extraction purification rhizoma paridis saponin I from Paris polyphylla |
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